ATE538069T1 - METHOD FOR THE CONTINUOUS PRODUCTION OF POLYCRYSTALLINE HIGH-PURITY SILICON GRANULES - Google Patents
METHOD FOR THE CONTINUOUS PRODUCTION OF POLYCRYSTALLINE HIGH-PURITY SILICON GRANULESInfo
- Publication number
- ATE538069T1 ATE538069T1 AT08155254T AT08155254T ATE538069T1 AT E538069 T1 ATE538069 T1 AT E538069T1 AT 08155254 T AT08155254 T AT 08155254T AT 08155254 T AT08155254 T AT 08155254T AT E538069 T1 ATE538069 T1 AT E538069T1
- Authority
- AT
- Austria
- Prior art keywords
- gas
- silicon
- bed
- fluidized
- reaction
- Prior art date
Links
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title abstract 9
- 239000008187 granular material Substances 0.000 title abstract 9
- 229910052710 silicon Inorganic materials 0.000 title abstract 9
- 239000010703 silicon Substances 0.000 title abstract 9
- 238000010924 continuous production Methods 0.000 title 1
- 238000000034 method Methods 0.000 title 1
- 239000007789 gas Substances 0.000 abstract 23
- 239000012495 reaction gas Substances 0.000 abstract 9
- 239000002245 particle Substances 0.000 abstract 8
- 238000010790 dilution Methods 0.000 abstract 6
- 239000012895 dilution Substances 0.000 abstract 6
- 238000006243 chemical reaction Methods 0.000 abstract 4
- 238000009826 distribution Methods 0.000 abstract 3
- 229910021420 polycrystalline silicon Inorganic materials 0.000 abstract 3
- 238000000151 deposition Methods 0.000 abstract 2
- 238000010438 heat treatment Methods 0.000 abstract 2
- 238000004519 manufacturing process Methods 0.000 abstract 2
- 239000000203 mixture Substances 0.000 abstract 2
- 206010024769 Local reaction Diseases 0.000 abstract 1
- 238000000071 blow moulding Methods 0.000 abstract 1
- 150000001875 compounds Chemical class 0.000 abstract 1
- 238000005094 computer simulation Methods 0.000 abstract 1
- 208000012839 conversion disease Diseases 0.000 abstract 1
- 238000005243 fluidization Methods 0.000 abstract 1
- 230000014759 maintenance of location Effects 0.000 abstract 1
- 229920005591 polysilicon Polymers 0.000 abstract 1
- XUGSDIOYQBRKGF-UHFFFAOYSA-N silicon;hydrochloride Chemical compound [Si].Cl XUGSDIOYQBRKGF-UHFFFAOYSA-N 0.000 abstract 1
- 239000000126 substance Substances 0.000 abstract 1
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 abstract 1
- 239000005052 trichlorosilane Substances 0.000 abstract 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
- C30B29/06—Silicon
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/02—Silicon
- C01B33/021—Preparation
- C01B33/027—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Silicon Compounds (AREA)
- Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)
Abstract
The method for producing highly pure polycrystalline silicon granulates by depositing a reaction gas of silicon granulates in a fluidized-bed reactor, comprises slightly fluidizing a lower zone (5) of a reactor chamber of a reactor by introducing a silicon-free gas by individual nozzles in the silicon granulates, directly connecting an upper zone of the reactor chamber with the lower zone, heating the zones over its external limiting wall, and injecting a silicon-containing reaction gas into the formed reaction zone by nozzles with high-speed than vertically arranged gas jet. The method for producing highly pure polycrystalline silicon granulates by depositing a reaction gas of silicon granulates in a fluidized-bed reactor, comprises slightly fluidizing a lower zone (5) of a reactor chamber of a reactor by introducing a silicon-free gas by individual nozzles in the silicon granulates, directly connecting an upper zone of the reactor chamber with the lower zone, heating the zones over its external limiting wall, and injecting a silicon-containing reaction gas into the formed reaction zone by nozzles with high-speed than vertically arranged gas jet. The local reaction gas jets surrounded by blow-forming fluidized-bed (2) are formed itself above the nozzles. The silicon-containing gas (11) decomposes itself at the particles surfaces within the fluidized-bed and leads for particle growth. The reaction gas is reacted almost up to the chemical equilibrium conversion before it reaches into the fluidized-bed wall or the fluidized-bed surface. The height of the lower zone is laid out so that no reaction gas flows back up to the nozzles for the dilution gas (12) for the fluidization of the lower zone and is blocked by the wall separator. The height of the lower zone is 50-300 mm. The dilution gas is supplied in a quantity to the nozzles. The gas speed in the lower zone is 1.2 to 2.3-times of the releasing gas speed. The maximum exhaust speed of the dilution gas from the nozzles is 20-200 m/s. The silicon-containing gases are used as reaction gas to the general compound of silicon hydrochloride (SiH xCl y) or mixtures of these gases are used as dilution gas with silicon-free gases. The mole fraction of trichlorosilane in the reaction gas is 0.2-0.8. The average mole fraction and the dilution gas from the lower zone over the entire reactor cross section is 0.15-0.4. The local gas speeds of the gases and/or the gas mixtures at the exit of the nozzle system are 1-140 m/s. The average gas speed in the reaction zone is 2-8 times of releasing gas speed. The minimum distance of the nozzles is selected to each other in such a way that the ratio of the nozzle distance to nozzle diameter is larger than 7.5. The exit speed at the annular nozzle is smaller than the exit speed at the central nozzle. The speed at the annular nozzle (V a n n u l a r n o z z l e) is 0.4-0.8 V c e n t r a l n o z z l e. The retention time of the gas in the upper zone of the fluidized-bed is 0.1-10 seconds. The bed temperature of the fluidized-bed is 890-1400[deg] C. The reactor pressure is positive pressure of 0-7 bar. The operation of the fluidized-bed has a stationary particle size distribution. The particles are 150-7000 mu m larger and the sauter diameter of the distribution is 850-1500 mu m. On-line exhaust gas analytics are used for the determination of the reaction conversion. The addition of the germ particles and the product distraction are steered in combination with the collection of the quantities on supplied reaction- and dilution gas and a computer model for particle population, so that the desired particle size distribution in the reactor and the quantity of granulates in the fluidized-bed are stable and stationarily kept over a long period of time. The undersize portion at the particles of less than 150 mu m lies under 0.1 mass percent, without necessary of additional classification step. The deposited polysilicon granulates have an expressed spherical form having sphericity value of 0.85 to 1 [-].
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE102007021003A DE102007021003A1 (en) | 2007-05-04 | 2007-05-04 | Process for the continuous production of polycrystalline high-purity silicon granules |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| ATE538069T1 true ATE538069T1 (en) | 2012-01-15 |
Family
ID=39789331
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| AT08155254T ATE538069T1 (en) | 2007-05-04 | 2008-04-28 | METHOD FOR THE CONTINUOUS PRODUCTION OF POLYCRYSTALLINE HIGH-PURITY SILICON GRANULES |
Country Status (8)
| Country | Link |
|---|---|
| US (1) | US8722141B2 (en) |
| EP (1) | EP1990314B1 (en) |
| JP (1) | JP4971240B2 (en) |
| KR (1) | KR101026815B1 (en) |
| CN (1) | CN101298329B (en) |
| AT (1) | ATE538069T1 (en) |
| DE (1) | DE102007021003A1 (en) |
| ES (1) | ES2376695T3 (en) |
Families Citing this family (61)
| Publication number | Priority date | Publication date | Assignee | Title |
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| DE102008000052A1 (en) | 2008-01-14 | 2009-07-16 | Wacker Chemie Ag | Method of depositing polycrystalline silicon |
| CN103058194B (en) | 2008-09-16 | 2015-02-25 | 储晞 | Reactor for producing high-purity particulate silicon |
| US8168123B2 (en) * | 2009-02-26 | 2012-05-01 | Siliken Chemicals, S.L. | Fluidized bed reactor for production of high purity silicon |
| EP2421659A1 (en) | 2009-04-20 | 2012-02-29 | Ae Polysilicon Corporation | A reactor with silicide-coated metal surfaces |
| TWI454309B (en) * | 2009-04-20 | 2014-10-01 | Jiangsu Zhongneng Polysilicon Technology Dev Co Ltd | Methods and system for cooling a reaction effluent gas |
| US20100266762A1 (en) * | 2009-04-20 | 2010-10-21 | Ben Fieselmann | Processes and an apparatus for manufacturing high purity polysilicon |
| US8075692B2 (en) * | 2009-11-18 | 2011-12-13 | Rec Silicon Inc | Fluid bed reactor |
| AT509388B1 (en) * | 2010-02-12 | 2012-06-15 | Andritz Tech & Asset Man Gmbh | FLOOD FLOOR FOR A FLUIDIZING APPARATUS |
| TW201142069A (en) * | 2010-03-19 | 2011-12-01 | Gt Solar Inc | System and method for polycrystalline silicon deposition |
| KR101329030B1 (en) | 2010-10-01 | 2013-11-13 | 주식회사 실리콘밸류 | Fluidized Bed Reactor |
| KR101057101B1 (en) * | 2010-10-12 | 2011-08-17 | (주)기술과가치 | Fluidized bed reactor for producing particulate polycrystalline silicon and polycrystalline silicon manufacturing method using the same |
| US20120100059A1 (en) | 2010-10-22 | 2012-04-26 | Memc Electronic Materials, Inc. | Production of Polycrystalline Silicon By The Thermal Decomposition of Trichlorosilane In A Fluidized Bed Reactor |
| US20120100061A1 (en) | 2010-10-22 | 2012-04-26 | Memc Electronic Materials, Inc. | Production of Polycrystalline Silicon in Substantially Closed-loop Processes |
| US8449848B2 (en) | 2010-10-22 | 2013-05-28 | Memc Electronic Materials, Inc. | Production of polycrystalline silicon in substantially closed-loop systems |
| CN102001660A (en) * | 2010-11-24 | 2011-04-06 | 天津大学 | Polysilicon reducing furnace with multiple gas outlets on chassis |
| US20120148728A1 (en) * | 2010-12-09 | 2012-06-14 | Siliken Sa | Methods and apparatus for the production of high purity silicon |
| US9156705B2 (en) * | 2010-12-23 | 2015-10-13 | Sunedison, Inc. | Production of polycrystalline silicon by the thermal decomposition of dichlorosilane in a fluidized bed reactor |
| KR101329033B1 (en) * | 2011-04-20 | 2013-11-14 | 주식회사 실리콘밸류 | Fluidized Bed Reactor |
| KR101356391B1 (en) * | 2011-04-20 | 2014-02-03 | 주식회사 실리콘밸류 | Apparatus for manufacturing polycrystalline silicon |
| KR101329035B1 (en) | 2011-04-20 | 2013-11-13 | 주식회사 실리콘밸류 | Fluidized Bed Reactor |
| KR101329032B1 (en) | 2011-04-20 | 2013-11-14 | 주식회사 실리콘밸류 | Apparatus for manufacturing polycrystalline silicon and method for manufacturing polycrystalline silicon using the same |
| CN107253723B (en) * | 2011-09-30 | 2020-06-26 | 各星有限公司 | Production of polycrystalline silicon by thermal decomposition of silane in a fluidized bed reactor |
| WO2013049325A1 (en) | 2011-09-30 | 2013-04-04 | Memc Electronic Materials, Inc. | Production of polycrystalline silicon by the thermal decomposition of silane in a fluidized bed reactor |
| DE102012206439A1 (en) | 2012-04-19 | 2013-10-24 | Wacker Chemie Ag | Polycrystalline silicon granules and their preparation |
| DE102012207505A1 (en) | 2012-05-07 | 2013-11-07 | Wacker Chemie Ag | Polycrystalline silicon granules and their preparation |
| US8875728B2 (en) | 2012-07-12 | 2014-11-04 | Siliken Chemicals, S.L. | Cooled gas distribution plate, thermal bridge breaking system, and related methods |
| TWI613231B (en) * | 2012-07-17 | 2018-02-01 | 陝西有色天宏瑞科矽材料有限責任公司 | A reactor system and method of polycrystalline silicon production therewith |
| DE102012212913A1 (en) | 2012-07-24 | 2014-05-15 | Evonik Industries Ag | Process for the preparation of alkenylhalosilanes and reactor suitable therefor |
| WO2014035878A1 (en) * | 2012-08-29 | 2014-03-06 | Hemlock Semiconductor Corporation | Tapered fluidized bed reactor and process for its use |
| US20140112832A1 (en) * | 2012-10-19 | 2014-04-24 | Rec Silicon Inc | Threaded nozzle and closable nozzle valve assembly |
| US9212421B2 (en) * | 2013-07-10 | 2015-12-15 | Rec Silicon Inc | Method and apparatus to reduce contamination of particles in a fluidized bed reactor |
| US9587993B2 (en) | 2012-11-06 | 2017-03-07 | Rec Silicon Inc | Probe assembly for a fluid bed reactor |
| CN105026029B (en) * | 2012-12-31 | 2017-12-22 | 爱迪生太阳能公司 | Improved Fluid Bed Reactor Operation by Optimizing Temperature Gradients with Particle Size Distribution Control |
| DE102013208071A1 (en) | 2013-05-02 | 2014-11-06 | Wacker Chemie Ag | Fluidized bed reactor and process for producing granular polysilicon |
| DE102013208274A1 (en) | 2013-05-06 | 2014-11-20 | Wacker Chemie Ag | Fluidized bed reactor and process for producing granular polysilicon |
| DE102013209076A1 (en) | 2013-05-16 | 2014-11-20 | Wacker Chemie Ag | A reactor for producing polycrystalline silicon and a method for removing a silicon-containing deposit on a component of such a reactor |
| US9580327B2 (en) | 2014-02-11 | 2017-02-28 | Rec Silicon Inc | Method and apparatus for consolidation of granular silicon and measuring non-metals content |
| CN104947187B (en) * | 2014-03-31 | 2018-03-23 | 新特能源股份有限公司 | A kind of preparation method of silicon chip foundry alloy |
| US9238211B1 (en) | 2014-08-15 | 2016-01-19 | Rec Silicon Inc | Segmented silicon carbide liner |
| US9446367B2 (en) | 2014-08-15 | 2016-09-20 | Rec Silicon Inc | Joint design for segmented silicon carbide liner in a fluidized bed reactor |
| US9662628B2 (en) | 2014-08-15 | 2017-05-30 | Rec Silicon Inc | Non-contaminating bonding material for segmented silicon carbide liner in a fluidized bed reactor |
| DE102014221928A1 (en) | 2014-10-28 | 2016-04-28 | Wacker Chemie Ag | Fluidized bed reactor and process for producing polycrystalline silicon granules |
| CN107250428A (en) * | 2014-12-23 | 2017-10-13 | 斯泰克有限责任公司 | Mechanical fluidized deposition systems and methods |
| DE102015209008A1 (en) * | 2015-05-15 | 2016-11-17 | Schmid Silicon Technology Gmbh | Process and plant for the decomposition of monosilane |
| DE102015216144A1 (en) * | 2015-08-24 | 2017-03-02 | Wacker Chemie Ag | Sintered polycrystalline silicon filter |
| DE102015224120A1 (en) * | 2015-12-02 | 2017-06-08 | Wacker Chemie Ag | Fluidized bed reactor and process for producing polycrystalline silicon granules |
| WO2017160121A1 (en) * | 2016-03-18 | 2017-09-21 | 주식회사 엘지화학 | Ultra-high temperature precipitation process for manufacturing polysilicon |
| DE102016204651A1 (en) | 2016-03-21 | 2017-09-21 | Wacker Chemie Ag | Crimp sleeves for the production of polysilicon granules |
| WO2018108258A1 (en) | 2016-12-14 | 2018-06-21 | Wacker Chemie Ag | Process for producing polycrystalline silicon |
| KR102096577B1 (en) * | 2016-12-29 | 2020-04-02 | 한화솔루션 주식회사 | polysilicon manufacturing reactor |
| EP3606874B1 (en) * | 2017-10-05 | 2021-03-24 | Wacker Chemie AG | Process for the preparation of chlorosilanes |
| TWI643683B (en) * | 2017-10-19 | 2018-12-11 | Scientech Corporation | Fluid supply device |
| JPWO2020213472A1 (en) * | 2019-04-18 | 2020-10-22 | ||
| EP3962861A1 (en) * | 2019-04-29 | 2022-03-09 | Wacker Chemie AG | Process for producing trichlorosilane with structure-optimised silicon particles |
| US10717061B1 (en) * | 2019-06-26 | 2020-07-21 | X Energy, Llc | Fluidized bed reactor system allowing particle sampling during an ongoing reaction |
| JP7478101B2 (en) * | 2019-09-05 | 2024-05-02 | パブリクノエ アクツィオネルノエ オブシチェストヴォ“ノヴォシビルスキー ザヴォッド シムコンシントラトフ” | Reaction chamber for the extraction of uranium dioxide powder from uranium hexafluoride using the reductive pyrohydrolysis method |
| KR102813955B1 (en) * | 2020-07-17 | 2025-05-27 | 와커 헤미 아게 | Method for producing polycrystalline silicon granules |
| WO2022111830A1 (en) * | 2020-11-30 | 2022-06-02 | Wacker Chemie Ag | Process for manufacturing silicon-containing materials |
| KR20240125024A (en) * | 2021-12-20 | 2024-08-19 | 와커 헤미 아게 | Method for producing silicon-containing material in a stirred tank reactor |
| KR102712596B1 (en) * | 2022-08-29 | 2024-09-30 | 오씨아이 주식회사 | Method for manufacturing silicon microparticles and silicon microparticles prepared by the same |
| KR20250101187A (en) * | 2023-12-27 | 2025-07-04 | 오씨아이 주식회사 | Method for manufacturing silicon microparticles, silicon microparticles manufactured thereby, and device for manufacturing silicon microparticles |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3963838A (en) | 1974-05-24 | 1976-06-15 | Texas Instruments Incorporated | Method of operating a quartz fluidized bed reactor for the production of silicon |
| US4651807A (en) * | 1985-03-13 | 1987-03-24 | Westinghouse Electric Corp. | Method and apparatus for cooling a high temperature waste gas using a jetting bed, fluidized bed technique |
| US4992245A (en) | 1988-03-31 | 1991-02-12 | Advanced Silicon Materials Inc. | Annular heated fluidized bed reactor |
| JPH02279513A (en) | 1989-04-20 | 1990-11-15 | Osaka Titanium Co Ltd | Production of high-purity polycrystal silicon |
| GB2271518B (en) * | 1992-10-16 | 1996-09-25 | Korea Res Inst Chem Tech | Heating of fluidized bed reactor by microwave |
| US6274191B1 (en) * | 1994-03-07 | 2001-08-14 | Medtronic, Inc. | Precise regulation of pyrocarbon coating |
| US5798137A (en) | 1995-06-07 | 1998-08-25 | Advanced Silicon Materials, Inc. | Method for silicon deposition |
| DE19735378A1 (en) * | 1997-08-14 | 1999-02-18 | Wacker Chemie Gmbh | Process for the production of high-purity silicon granules |
| DE19948395A1 (en) | 1999-10-06 | 2001-05-03 | Wacker Chemie Gmbh | Fluidized bed reactor with radiative heating, useful for producing high purity polycrystalline silicon, e.g. for electronics, by passing silicon-containing gas over hot silicon particles |
| US6827786B2 (en) | 2000-12-26 | 2004-12-07 | Stephen M Lord | Machine for production of granular silicon |
| AU2002329626A1 (en) * | 2002-07-22 | 2004-02-23 | Stephen M. Lord | Methods for heating a fluidized bed silicon manufacture apparatus |
| DE10359587A1 (en) * | 2003-12-18 | 2005-07-14 | Wacker-Chemie Gmbh | Dust- and pore-free high-purity polysilicon granules |
| DE102005042753A1 (en) * | 2005-09-08 | 2007-03-15 | Wacker Chemie Ag | Method and device for producing granular polycrystalline silicon in a fluidized bed reactor |
| JP4716372B2 (en) | 2005-09-27 | 2011-07-06 | コバレントマテリアル株式会社 | Silicon wafer manufacturing method |
| KR100756310B1 (en) * | 2006-02-07 | 2007-09-07 | 한국화학연구원 | High Pressure Fluidized Bed Reactor for Particle Polycrystalline Silicon Production |
| KR100661284B1 (en) * | 2006-02-14 | 2006-12-27 | 한국화학연구원 | Polysilicon Production Method Using Fluidized Bed Reactor |
| KR100783667B1 (en) * | 2006-08-10 | 2007-12-07 | 한국화학연구원 | Method and apparatus for manufacturing particulate polycrystalline silicon |
-
2007
- 2007-05-04 DE DE102007021003A patent/DE102007021003A1/en not_active Withdrawn
-
2008
- 2008-04-28 ES ES08155254T patent/ES2376695T3/en active Active
- 2008-04-28 EP EP08155254A patent/EP1990314B1/en active Active
- 2008-04-28 AT AT08155254T patent/ATE538069T1/en active
- 2008-04-29 US US12/111,291 patent/US8722141B2/en active Active
- 2008-05-02 KR KR1020080041232A patent/KR101026815B1/en active Active
- 2008-05-04 CN CN2008100928166A patent/CN101298329B/en active Active
- 2008-05-07 JP JP2008121383A patent/JP4971240B2/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN101298329B (en) | 2012-01-04 |
| DE102007021003A1 (en) | 2008-11-06 |
| EP1990314B1 (en) | 2011-12-21 |
| ES2376695T3 (en) | 2012-03-16 |
| JP2008273831A (en) | 2008-11-13 |
| KR20080098322A (en) | 2008-11-07 |
| US8722141B2 (en) | 2014-05-13 |
| EP1990314A2 (en) | 2008-11-12 |
| US20080299291A1 (en) | 2008-12-04 |
| JP4971240B2 (en) | 2012-07-11 |
| EP1990314A3 (en) | 2009-08-12 |
| CN101298329A (en) | 2008-11-05 |
| KR101026815B1 (en) | 2011-04-04 |
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